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Dunyong Deng
Linköping 2018
Cover image: A fracture surface of EBM IN718 after tensile test at room temper-
ature.
During the course of research underlying this thesis, Dunyong Deng was enrolled
in Agora Materiae, a multidiciplinary doctoral program at Linköping University,
Sweden.
© Dunyong Deng
ISBN 978-91-7685-383-2
ISSN 0280-7971
iii
Post heat treatment can slightly increase the mechanical strength compared to the
as-manufactured condition but does not alter the anisotropy. SLM IN718 shows
significantly different microstructure and mechanical properties to EBM IN718.
The as-manufactured SLM IN718 has very fine dendritic microstructure and Laves
phases in the interdendrites, and is “work-hardened” by the residual strains and
dislocations present in the material. Mechanical properties are different between
horizontally and vertically built samples, and heat treatment can minimize this
difference. Results from this licentiate thesis provide the basis for the further
research on the cyclic mechanical properties of EBM and SLM IN718, which would
be the focus of following phase of the Ph.D. research.
iv
Populärvetenskaplig sammanfattning
Additiv tillverkning (AM), även känt som 3D-printning, har väckt ett stort intresse
inom flera olika sektorer så som flyg-, energi-, fordon- och medicinsk-industri på
grund av dess möjlighet att tillverka komponenter som antingen är väldigt kost-
samma eller omöjliga att tillverka med konventionella processer. Bland de olika ad-
ditiva tillverkningsprocesserna för metallkomponenter är elektronstrålesmältning
(EBM) och selektiv lasersmältning (SLM) två av de mest använda pulverbädds-
baserade processerna och de har visat stor potential för tillverkning av avancer-
ade kritiska komponenter, såsom turbinblad och anpassade medicinska implantat.
Framtiden för EBM och SLM är utan tvekan mycket lovande, men för att fullt ut
kunna realisera processernas möjligheter finns det fortfarande många utmaningar
att övervinna.
Inconel 718 (IN718) är en nickelbaserad superlegering med en god kombination
av bra mekaniska egenskaper och låg kostnad. Även om IN718 nu mestadels an-
vänds som ett turbinskivmaterial, så var det huvudsakliga motivet för att utveckla
IN718 att övervinna den låga svetsbarheten som fanns hos många superlegeringar
på 1960-talet. Fördelen men IN718 är den långsamma utskiljningshastigheten hos
förstärkningsfaserna γ ′ /γ ′′ vilket ger ett högt motstånd mot varmsprickor vid svet-
sning och vid den efterföljande värmebehandlingen. Med tanke på likheten mellan
AM och svetsning så har IN718 tillämpats i relativt stor utsträckning för met-
alliska AM-processer och redan befintlig kunskap kan underlättat förståelsen för
relationen mellan process-mikrostruktur-egenskaper även för AM.
Arbetet som presenteras i denna licentiatavhandling syftar till att bättre förstå
mikrostrukturer och mekaniska egenskaper för EBM och SLM IN718, något som
ännu inte är systematiskt undersökt. Mikrostrukturer för EBM och SLM IN718
har karakteriserats med svepelektronmikroskopi (SEM) och transmissionselektron-
mikroskopi (TEM) samt korrelerats till processbetingelserna. Statiska mekaniska
egenskaper (t ex Vickers-mikrohårdhet och dragprovning) har också undersökts
och kopplats till mikrostrukturutvecklingen före och efter olika värmebehandlin-
gar.
v
För EBM IN718 visar resultaten att mikrostrukturen inte är homogen utan
beroende på läge i komponenten. Dessutom är de anisotropa mekaniska egen-
skaperna troligen en konsekvens av porositeter uppradade och orienterade in en
viss riktning snarare än kristallografisk textur. Eftervärmebehandling kan öka den
mekaniska hållfastheten något jämfört med den direkt efter tillverkning, men detta
ändrar inte anisotropin. SLM IN718 visar en signifikant skillnad i mikrostruk-
tur och mekaniska egenskaper jämfört med EBM IN718. Direkt efter tillverkning
har SLM IN718 en mycket fin dendritisk mikrostruktur med Laves-faser mellan
dendriterna och kan betraktas som kallbearbetat på grund av den höga närvaro
av restspänningar och dislokationer som finns i materialet. De mekaniska egen-
skaperna är olika mellan horisontellt och vertikalt byggda prover, och värmebe-
handling kan minimera denna skillnad. Resultat från denna licentiatavhandling
utgör grunden för fortsatt forskning kring de cykliska mekaniska egenskaperna
hos EBM och SLM IN718, vilket kommer att vara i fokus under den avslutande
delen av detta doktorandprojekt.
vi
Acknowledgements
First and foremost, I would like to acknowledge Chinese Scholarship Council (CSC)
for the financial support, and Professor Ru Lin Peng for offering me this Ph.D.
position, without which I would never have had the chance to present this work
here.
Especially, I am indebted to my supervisor Professor Johan Moverare. You
have provided me with every bit of advice, support, help and encouragement that
guided me to move on. It is my greatest honour to have you as my supervisor,
and I believe working with you will be the most valuable experience in my life.
Again, I would like to thank my co-supervisor Professor Ru Lin Peng. Thank
you for sharing microstructural characterization skills and knowledge with me, and
the fruitful discussions in the past years. Your diligence and devotion set a good
example of a good researcher to me.
A collective acknowledgement goes to my colleagues at the Division of Engi-
neering Materials, Linköping University. Thanks to the positive work atmosphere,
the knowledge about research and life you shared with we, I have survived the dark
and cold winters in Sweden. I am also grateful to all the administrators and techni-
cians: Ingmari Hallkvist, Annethe Billenius, Rodger Romero Ramirez and Patrik
Härnman, without you everything would have never gone so smoothly.
Further, I would like to express my gratitude to Professor Per-Olof Holtz for
managing the Agora Materiae Graduate School, and to Professor Per Persson for
teaching me how to operate TEM. To Hans Söderberg from Sandvik Machining
Solutions, Håkan Brodin from Siemens Industrial Turbomachinery AB, Chamara
Kumara and Paria Karimi Neghlani from University West, it is my pleasure to
have collaborations with you and I am looking forward to further collaborations in
the future. I am also highly obliged to Sandvik Machining Solutions, Sweden and
Siemens AG, Germany for their generosities in providing samples for this work.
我自认为是一个不善表达的人,写这段致谢时总怕遗漏了谁,不敢轻易点名,
也怕寥寥数语词不达意,但懂我的终将能在字里行间对号入座。求学在外多年,我
最感谢我的父母亲和姐姐姐夫,你们替我承担了太多的艰辛,让我在本该养家糊
vii
口的年纪依然能投身学术;俊沅、星翰和星豫,你们守护着我为人处世的一份童
真。我要感谢我在林雪萍的小伙伴们,背井离乡的苦辣酸甜幸得有你们的分担,尤
其感谢张丕敏,减肥大业一直没有荒废。有太多金属所的同学要感谢,即使我们
天各一方,但你们依然愿意算好时差跟我讨论学术聊聊近况,或者只是毫无营养
地互黑,这些情谊是我一辈子最宝贵的财富,不要太想我,但我很想大家。
Dunyong Deng
邓敦勇
Linköping, January 2018
viii
Contents
Abstract iii
Acknowledgements vii
2 Inconel 718 7
2.1 History and use . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
2.2 Alloying elements in nickel-base superalloys . . . . . . . . . . . . . 8
2.3 Phases and their properties in IN718 . . . . . . . . . . . . . . . . 8
2.3.1 γ ′ and γ ′′ . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10
2.3.2 δ . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
2.3.3 MC carbide . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
2.3.4 Laves . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12
2.4 Solidification metallurgy . . . . . . . . . . . . . . . . . . . . . . . . 13
2.5 Heat treatments . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
2.5.1 Wrought IN718 . . . . . . . . . . . . . . . . . . . . . . . . . 14
2.5.2 Cast IN718 . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
2.5.3 Powder metallurgy (P/M) IN718 . . . . . . . . . . . . . . . 16
2.5.4 Additively manufactured IN718 . . . . . . . . . . . . . . . . 16
2.6 Anisotropy . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
ix
3.3.2 Surface roughness . . . . . . . . . . . . . . . . . . . . . . . 23
3.4 Materials manufactured with EBM . . . . . . . . . . . . . . . . . . 24
3.5 Future work . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24
6 Experimental methods 37
6.1 Materials . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37
6.1.1 EBM IN718 . . . . . . . . . . . . . . . . . . . . . . . . . . . 37
6.1.2 SLM IN718 . . . . . . . . . . . . . . . . . . . . . . . . . . . 37
6.2 Microstructure characterization . . . . . . . . . . . . . . . . . . . . 38
6.2.1 Metallographic preparation . . . . . . . . . . . . . . . . . . 38
6.2.2 Scanning electron microscopy . . . . . . . . . . . . . . . . . 39
6.2.3 Transmission electron microscopy . . . . . . . . . . . . . . . 39
6.2.4 Residual stress measurement . . . . . . . . . . . . . . . . . 39
6.3 Mechanical test . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39
6.3.1 Hardness test . . . . . . . . . . . . . . . . . . . . . . . . . . 39
6.3.2 Tensile test . . . . . . . . . . . . . . . . . . . . . . . . . . . 39
8 Conclusion 45
9 Future work 49
Bibliography 51
Paper II 87
x
Part Part I:
若廣學,懼其繁,但略說,能知源。
凡訓蒙,須講究,詳訓詁,明句讀。
《三字經》
1
CHAPTER 1
Introduction
1.1 Background
Additive Manufacturing (AM), also known as 3D printing, is a group of manu-
facturing processes that build components in an additive layer-by-layer or drop-
by-drop fashion,which is able to obtain net shape components. Essentially, AM
can offer great freedom to design and manufacture geometrically complex struc-
tures that are either impossible or considerably expensive by conventional pro-
cesses, which rely on removing materials from monoliths. Given that, over the
past decade, AM has attracted significant interest in manufacturing of critical
metallic components with complex geometry in turbines and engines, as well as
customised orthopaedic implants [1]. The development of the AM industry has
shifted the focus from rapid plastic prototyping to metallic ready-for-use compo-
nents. Unlike the plastic material, to additively manufacture metallic components,
the interaction of the material and the melting source is relatively complicated
and has not been well-understood. On the other hand, the high-end applications
of metallic AM components are rather defect-intolerant, which require an opti-
mization of the process to get desired microstructures and mechanical properties.
The future of AM is doubtlessly promising, but to fully realize its potential, the
process-microstructure-properties relationship needs to be but not yet systemati-
cally studied .
3
Introduction
IN718 is being used intensively in gas turbines and aero engines for discs and
frames. Due to IN718’s excellent weldability and similarity of the AM and weld-
ing precesses, IN718 has been widely applied in metallic AM fields to understand
the fundamentals of AM processes. Electron beam melting (EBM) and Selective
laser melting (SLM) are two of the most widely used AM processes for metallic
components, and have very different processing conditions which would result in
quite different microstructures and mechanical properties. The general aims of the
present research are to characterize the microstructures and mechanical proper-
ties of IN718 manufactured by EBM and SLM, and the effects of heat treatments
on microstructure evolutions and mechanical properties. In the present licentiate
thesis, the main focus is placed on correlating the microstructures and monotonic
mechanical properties (e.g., microhardness and tensile properties) with the pro-
cesses and post heat treatments, based on which the cyclic mechanical tests would
be performed in the future research. More specifically, this thesis addresses the
following research questions:
4
Introduction
In Part I Background & Theory, the research project and the research ques-
tions aimed to address is first introduced to help the readers to get a picture of
this licentiate thesis. Then, the more specific sections reviewing the Inconel 718,
EBM, SLM, EBM and SLM IN718 are provided to give fundamental details on
the investigating subjects. Following, the experimental methods are given as well
as a summary of the papers included. The conclusions of the researches present
in this thesis are also listed, based on which the future work is planed for the next
phase of my Ph.D. research.
In Part II Papers Included, three journal papers that address the aforemen-
tioned research questions are presented.
5
Introduction
6
CHAPTER 2
Inconel 718
Thanks to its good mechanical properties and low cost, Inconel 718 (IN718) is never
out of the spotlight and has earned success in a wide range of applications, such as
aircraft and land-based gas turbine engines, cryogenic tankage and liquid fuelled
rockets. In this chapter, a review on IN718’s history & use, chemical composi-
tion and phases, solidification metallurgy, post heat treatments, and anisotropy is
provided. This review will surely offer insight into further discussion of additively
manufactured IN718.
7
Inconel 718
and cryogenic structures due to its excellent strength and aqueous corrosion resis-
tance at ambient and low temperature [5, 6]. As a result, IN718 is the most widely
used superalloy, accounting for 35 % of all superalloy production in the late 1980s
[5], and over 50 % of the superalloy content in some engines [2].
Element Ni Cr Mo, W Al Ti Co Nb Ta Re
Range, wt.% Bal. 5-25 0-12 0-6 0-6 0-20 0-5 0-12 0-6
8
Table 2.2. Alloying element effects in nickel-base superalloys
Element Effects
Cr Solid-solution strengthener, M7 C3 and M23 C6 carbides former, improve oxidation and hot corrosion resistance
Co Solid-solution strengthener, raises solvus temperature of γ ′ Ni3 (Al,Ti)
Al Strengthening phase γ ′ Ni3 (Al,Ti) former, improve oxidation and hot corrosion resistance
Ti Strengthening phase γ ′ Ni3 (Al,Ti) former former
Nb Strengthening phase γ ′′ Ni3 Nb former, MC and M6 C carbides former,
9
Fe Solid-solution strengthener,
Mo Solid-solution strengthener, MC, M23 C6 and M6 C carbides former
W Solid-solution strengthener, MC, M23 C6 and M6 C carbides former
Ta Solid-solution strengthener, MC carbide former, improve creep properties
Re Solid-solution strengthener, retard γ ′ coarsening
C M(C,N) carbonitrides former, grain-boundary strengthener
N M(C,N) carbonitrides former
B Grain-boundary strengthener, improve creep properties and rupture strength
Inconel 718
Inconel 718
Table 2.3. IN718 composition per Aerospace Material Specifications (AMS) 5383
IN718 consists of the matrix phase γ and a variety of secondary phases. Since
IN718 is a precipitate-strengthened superalloy, the presence and distribution of
secondary phases in the matrix are the key to determining IN718’s microstructure
and properties. Table 2.4 summarized the crystal structures and chemical formulas
of the commonly encountered phases in IN718.
2.3.1 γ ′ and γ ′′
In IN718 both γ ′ and γ ′′ are present and coherent with the γ matrix. Comparing
the D022 crystal structure of γ ′′ to the L12 crystal structure of γ ′ , the lattice
parameter a of γ ′′ almost equals to that of γ ′ , but the lattice parameter c is
roughly doubled, by which γ ′′ is named. Both γ ′ and γ ′′ can strengthen the γ
matrix by the following strengthening mechanisms [7]:
When IN718 is nearly peak aged, the coherency strain hardening caused by the
lattice mismatch confers principally strength to this superalloy [9, 10]. In IN718,
γ ′ phase precipitates in a spherical morphology with a lattice mismatch of less
than 0.5 % [11]. The presence of γ ′′ is in a disk morphology, and the tetragonal
10
Inconel 718
lattice distortion (c/a = 2.04) results in considerable coherency strain [12]. The
lattice mismatch between γ ′′ and γ matrix is reported as 2.86 % [10]. The relative
volume fraction ratio of γ ′′ to γ ′ is about 3 [10, 13, 14], and Li et al. [14] suggested
that heat treatment does not notably influence this fraction ration. The volume
fraction of γ ′′ in peak aged IN718 is about 15 % while γ ′ accounts for just 4%
[13, 15]. Therefore, though γ ′ phase does contribute to the strength of IN718,
the principal strengthening is actually from γ ′′ phase due to both higher lattice
mismatch and volume fraction.
2.3.2 δ
The γ ′′ phase in IN718 is metastable and can covert to the thermodynamically
stable δ phase with a needle or plate-like morphology under thermal exposure. δ
phase is incoherent with γ matrix, conferring rarely strength to the matrix when
present in large quantities; on the contrary, the precipitation of δ phase would be
at the expense of Nb, which associates with the loss of γ ′′ and therefore strength [7,
16]. The conversion from γ ′′ to δ is accelerated when the thermal exposure is over
650 ◦ C, which limits the main applications of IN718 under 650 ◦ C [17, 18]. The
formation of δ is believed as a result of the excessive coherent mismatch between
γ ′′ and γ matrix, and can be retarded by increasing the Al/Ti ratio and/or the Al
+ Ti content in IN718 [19]. With higher Al/Ti ratio and/or Al + Ti content, the
size of γ ′′ is reduced as well as the lattice mismatch between the γ ′′ and γ matrix,
therefore decreasing the driving force to form δ.
However, δ phase has favourable effects on the microstructure and mechanical
properties under certain circumstances. Over 4% of δ phase at grain boundaries
can efficiently inhibit the grain growth during heat treatment and working, which
is an important aspect of current high-strength IN718 production [7, 20]. Globular
grain boundary δ phase is beneficial to stress rupture [21, 22] and creep [21–23]
properties, since the δ phase retards the intergranular crack propagation which is
the predominant failure mechanism. The effects of grain boundary δ on fatigue
properties are dependent on the fatigue fracture mode: having no influence on high
cycle fatigue crack growth rate at 650 ◦ C because of the transgranular fracture
mode [23, 24], while improving the resistance to crack propagation along boundary
under low cycle fatigue test where fracture is intergranular [25].
2.3.3 MC carbide
The predominant carbide phase in IN718 is Nb-rich MC phase, because the rel-
atively high content of Nb promotes the formation of MC type carbide. Ti also
incorporates in this MC carbide, resulting in its lattice parameter ranging between
NbC and TiC phase but closer to the former [26]. Therefore, the primary MC car-
bide is denoted as NbC or (Nb,Ti)C in IN718. The primary MC carbide is mostly
in discrete blocky shape and distributes in a non uniform manner within the grains
as well as at the grain boundaries [26, 27].
• Intragranular MC carbide: The role of intragranular MC carbide in IN718 is
less well documented. Generally, intragranular carbide can impede basic dis-
11
Inconel 718
location movement but confer very small strength to the matrix, comparing
the principal strengthening from γ ′′ precipitation. In addition, this carbide at
a component’s surface may be precracked or oxidized under thermal stresses,
causing a unfavourable notch effect and degrading fatigue properties [7].
• Grain boundary MC carbide: MC carbides precipitated at grain boundaries
promote the fracture mode transiting from transgranular to intergranular at
room temperature [26]. During plastic deformation the stress would concen-
trate at the carbide and matrix interface, causing microcrack to relax the
localized stress. When the MC carbides closely distribute along the grain
boundaries, the microcracks would easily joint up and facilitate intergranular
fracture. Though their effects on mechanical behaviour at elevated temper-
ature have been rarely reported, it is expected that grain boundaries MC
carbides discretely distributed and with appropriate size would restrict the
grain boundary movement and give better rupture life.
As aforementioned, MC carbide being beneficial or detrimental to mechan-
ical properties would depend on the size, distribution, precrack, oxidation and
mechanical test condition. Mitchell et al. [28] concluded that TiN nitride can
substantially promote the precipitation of MC carbide by acting as heterogeneous
nucleation site, which would provide a potential of manipulating MC carbide dis-
tribution to optimize the mechanical properties.
2.3.4 Laves
Laves phase is a brittle intermetallic topologically close packed (TCP) phase, and
is detrimental to mechanical properties. The formation of Laves phase is a result
of Nb, Si and Mo segregation during solidification, where these alloying elements
are rejected from the dendrites into the interdendrites [29, 30]. Chang et al. [31]
suggested that the relatively high contents of Cr and Fe in IN718 are the neces-
sary condition for Laves phase, aside from the segregation of Nb. The chemical
composition of Laves might differ with solidification condition, but is generally re-
ferred as (Ni,Fe,Cr)2 (Nb,Mo,Ti). In addition to its brittle nature, Laves depletes
the matrix of Nb and the principal strengthening γ ′′ phase. Schirra et al. [32]
summarized the effects of laves phase on the mechanical properties of wrought
and cast+hot isostatic pressing (HIP) IN718 as following:
12
Inconel 718
In addition, though the IN718 is reputed for good wedablitiy in the context of
its resistance to strain age cracking, the heat affected zone (HAZ) liquation crack-
ing/microfissuring is still a major concern for IN718 during welding. During the
heating cycles of welding, the low-melting-point Laves phase at grain boundaries
can be liquated, forming grain boundary liquid. With the development of thermal
stress during the cooling cycles of welding, the liquated grain boundaries are easily
torn apart, leading to the hot cracks/miscrofissures [33, 34].
• At low and intermediate cooling rates (0.25 ◦ C/s and 55.4 ◦ C/s respectively),
the solidification sequence is basically in good agreement with Knorovsky’s
solidification diagram, but there might be a reaction L+NbC→γ+Laves at
1160 ◦ C.
Obviously, the cooling rate significantly affects the diffusions of alloying ele-
ments and therefore the formations and growths of phases. Tailoring the thermal
13
Inconel 718
14
Inconel 718
treatment details and applicable AMS specifications are summarized in Table 2.5.
STD1 is the standard heat treatment for aerospace applications, gas turbine disks
for instance, producing high rupture properties, room-temperature tensile strength
and fatigue strength. For the tensile-limited applications, STD2 is preferred since
it produces the best transverse ductility in heavy sections, impact strength and
low-temperature notch tensile strength. Note that, all the grain boundary δ phases,
pinning the grain boundaries and providing the notch ductility, would be dissolved
by STD2, which would result in notch brittleness in stress rupture [7]. If a high-
quality billet is used as the starting material and then forging is done below the
δ solvus, direct ageing (DA) heat treatment is recommended for obtaining the
highest tensile properties though a slight loss in stress-rupture capability [7].
15
Inconel 718
Table 2.6. Standard heat treatment for cast IN718 per AMS 5383
16
Inconel 718
hot isostatic pressing treatments. Establishing the actual heat treatment should
be as agreed between the component supplier and purchaser.
Table 2.7. Heat treatment recommended for powder-bed AM IN718 per ASTM F3055
2.6 Anisotropy
Single-crystal or columnar-grained nickel-base superalloy is widely recognized as
elastically anisotropic, presenting different elastic properties when mechanical load-
ings are parallel to different crystallographic orientations [3]. As mentioned, IN718
is predominantly used in the polycrystalline wrought form, which is isotropic since
the large number of randomly orientated grains average out the elastic differences.
However, the additively manufactured IN718 is reported to be strongly textured
with ⟨001⟩ crystallographic orientation parallel to the building direction. Elas-
tic anisotropy of Ni (similar anisotropic behaviours are demonstrated nickel-based
superalloys) is reviewed in general terms herein, providing the fundamental knowl-
edge for anisotropic tensile properties discussed in the later chapters. For pure Ni,
the ⟨001⟩ has the least elastic modulus 125 GPa, while the ⟨111⟩ has the high-
est elastic modulus 294 GPa, with the ⟨110⟩ between the two limits (220 GPa);
for polycrystalline Ni, the elastic modulus is measured as 207 GPa at room tem-
perature [3]. These anisotropic elastic properties strongly influence the low cycle
fatigue performance: better fatigue properties is associated with the elastically
soft directions, such as ⟨001⟩, than the elastically stiff directions, such as ⟨111⟩,
because of both the greater elastic strain available to drive the fatigue process and
higher yield stress along the elastically soft directions [3].
17
Inconel 718
18
CHAPTER 3
3.1 Introduction
EBM is a powder-bed fusion (PBF) process that uses electron beam to selectively
melt the defined geometries at each layer and simultaneously fuses with previously
solidified layers in a powder bed, by which method a 3D part is built. The use of
an electron beam as the energy source offers specific advantages to this process.
To enable the electron beam to work appropriately, high vacuum is maintained
throughout the process, making EBM particularly suitable for manufacturing the
chemical-sensitive materials, e.g., titanium. With the electromagnetic lenses, the
electron beam can be focused or defocused to adjust the energy density for heating
or melting purposes. In addition, the state-of-the-art deflection electronics enables
the extremely rapid movement of electron beam within the building area, allow-
ing melting at multiple points simultaneously and achieving high melting capacity
and high productivity[46]. Further, it is worth mentioning that with the rapid
19
Electron beam melting
movement and defocus of the electron beam, the entire powder bed is heated and
maintained at an relatively high building temperature throughout the process, pro-
ducing the components free from residual stresses. On the other hand, the nature
of electron beam limits this process to conductive materials, since only conductive
materials can be heated by absorption of the energy carried by accelerated elec-
trons. In addition, inappropriate electrostatic charges in powders might lead to
an undesirable smoke phenomenon, which would suddenly cause the uncontrolled
repulsion/blowing of the powders and even process instabilities/termination [47,
48]. The detailed process will be given in the following sections.
3.2 Process
Fig. 3.1b illustrates the typical building cycle of an EBM process. A base plate is
first preheated slightly above the building temperature, before applying the first
layer of powder. As shown in Fig. 3.1b, for each building cycle, the base plate is
lowered and a new layer with a identical thickness of powder is laid on the top,
then the electron beam scans over this powder layer to consolidate the powders in
a predefined pattern. Note that the scanning of electron beam is firstly to preheat
and slightly sinter the current powder layer, then melt the current powder layer
and form a solid layer of the build. This cycle would be repeated until the build
is finished. After the building process is finished, the whole powder bed starts
cooling down itself. Accelerated the cooling is optional by injecting appropriate
amount of helium into the chamber.
(a) (b )
Figure 3.1. (a) Schematic configuration of an Arcam EBM machine [49], (b) schematic
building cycle of an EBM process [45].
20
Electron beam melting
3.2.2 Preheating
A preheating step, during which the electron beam is defocused and scans over
the powder layer several times, is performed before this powder layer is actually
melt and fused together. This is to slightly sinter the powders for better electric
conductivity and process stability, and to maintain the relatively high building
temperature within the whole building chamber [45].
Sintering is a solid state process that atoms at the particle interfaces diffuse to
the contiguous particles and form a “neck”, binding them together at the temper-
ature between half melting point and full melting point [56]. As a result of this
slightly sintering, the electric conductivity is improved compared to the loosely
stacked state, and the smoke phenomenon is therefore efficiently prevented [57].
A partial pressure of helium (4× 10−3 mbar) is also introduced into the vacuum
chamber to prevent smoke [46, 58]. When the entire process is finished, the build
will be embedded within a slightly sintered powder bed. The sintered powders can
be easily removed by sand blasting, and with appropriate sieving these powders
can be nearly completley recycled [45].
As mentioned, to slightly sinter the powder bed, the preheating temperature
have to be over half melting point. Therefore, the powder bed is maintained at
relatively high temperature throughout the process. For instance, for Ti6Al4V it
is typically between 550 to 700 ◦ C [58–60], and for IN718 it can be over 900 ◦ C
[61, 62]. This leads to mostly full in-situ stress relief and no residual stress in the
as-manufactured microstructure [63].
21
Electron beam melting
3.2.3 Melting
Melting is, after the preheating stage, to fully melt the powders and fuse them
together to form a solid component as designed. During the melting stage, two
scanning strategies, namely contour and hatch, are typically applied: contour is
to “draw” the frame of the build, while hatch is to “fill in” the interiors of the
build. Contour strategy uses the MultiBeam technology that splits the electron
beam into multiple spots and rapidly “draw” the frame, enabling optimization of
surface finish, precision and build speed simultaneously [46, 64]. Differently, hatch
strategy scans continuously the beam in a forwards-and-backwards pattern at each
layer, and the scanning direction is rotated by certain angel between each layer.
The process parameters, such as beam power, beam focus offset, beam velocity, line
offset (the distance between two adjacent scanning passes), are different with these
two scanning strategies, resulting in considerably different thermal conditions [65]
and therefore microstructures [66, 67].
3.3 Defects
As mentioned, the powder bed of the EBM process is maintained at relatively
high temperature, which leads to every low residual stresses in the as-manufactured
microstructures. Therefore, unlike the selective laser melting (SLM) process where
residual stress is the major concern for causing distortion and delamination, the
common defects in as-manufactured EBM components are porosity and surface
roughness.
3.3.1 Porosity
Typical porosities found in EBM builds are shown in Fig. 3.2. Porosity can be
catalogued as process-induced (Fig. 3.2a and b) and powder-induced (Fig. 3.2c
and d).
The process-induced porosity, referred as lack of fusion, is formed due to the
unoptimized process parameters, specifically inappropriate energy input [61]. This
kind of porosity is mostly irregular in shape and size varies from micrometer to
millimetre.
• Too much energy input would lead to spatter ejection, where a region of
powder is though fully melt but the melt is spattered away. As a result, lack
of melt to bond the desired melt region.
22
Electron beam melting
(a) (b)
(c) (d)
Figure 3.2. Examples of porosity defects in EBM Ti6Al4V builds: (a) continuous
beam tripping resulting in unconsolidated region progressing with build (arrow); (b) un-
melted pocket; (c) build flaw revealed in grinding and polishing sample; (d) hemispherical
(spherical) gas void [68].
gas atomized powders, despite the high vacuum atmosphere in the EBM chamber,
cannot necessarily escape from the melt but embed in the resulted microstructure
due to the rapid solidification process [66, 69], as seen in Fig. 3.2d.
The presence of porosities is detrimental to the mechanical properties, espe-
cially for the crack initiation and propagation resistances. Therefore, either tuning
the process parameters or improving powder the feedstock quality can reduce the
porosities during the process. On the other hand, HIP is widely applied to the
as-manufactured materials to improve density. HIP can significantly reduce the
porosities, but still cannot result in 100% dense microstructure [70]. HIP re-
duces/eliminates the process-induced porosities [71], but might not close those
gas-trapped pores since the trapped gas can still “prop up” the pores [72].
23
Electron beam melting
et al. [45] suggested that the coarser powder, thicker powder layer and larger beam
size lead to higher EBM surface roughness than that of SLM. Though post surface
machining is able to improve the surface condition for simple-geometry builds, it
offers no solutions for complex-geometry components.
24
Electron beam melting
25
Electron beam melting
26
CHAPTER 4
4.1 Introduction
First of all, Selective Laser Sintering (SLS), Direct Metal Laser Sintering (DMLS)
and Selective Laser Melting (SLM) follow essentially the same process philosophy
and procedure, as shown in Fig. 4.1. After the component’s 3D model has been
processed and transferred to the laser-base AM machine, the building process
starts with applying a thin layer of powder on the building base plate. A laser
beam is then used to melt the powders at the locations defined by design data for
the current layer, followed by lowering the base plate and applying a new layer of
powder with the identical thickness on the top. Once again, the laser beam melts
the powders at the predefined locations and fuses them with the previous layers.
This cycle is repeated until the component is finished as designed, after which the
component is removed from the loose powder bed.
27
Selective laser melting
Figure 4.1. General process procedure of laser-base powder-bed fusion (PBF) additive
manufacturing technologies. [90]
28
Selective laser melting
these nomenclatures don’t really reflect the differences in their abilities and
applications.
4.2 Process
The typical process cycle for SLM is as illustrated in Fig. 4.1. If compared
with the EBM process cycle, one can find that there is not a top down laser-
beam preheating stage before melting the powder. That can be attributed to the
relatively low power and small laser beam size, which can not efficiently preheat the
whole powder bed and maintain it at a elevated temperature. Thus, to preheat the
base plate, a resistive heat module is commonly installed underneath the building
platform [96]; to preheat the powder bed before melting stage, an extra laser source
is optional with certain systems [97].
Another thing worth to note is that during the melting stage, contour and
hatch scanning parameters are normally applied to draw the “skin” and fill in the
interior volume, respectively, as that in EBM process. Differently, contour followed
or following by hatch can vary from research to research [98, 99]. And the contour
is generally associated with lower power and lower scanning speed to improve the
geometry accuracy and roughness, while the hatch is adjusted to higher power and
higher scanning speed to increase the productivity [98, 100].
After the building process is finished, the component is embedded within a
loosely aggregated powder bed and it can be easily removed from the powder bed.
However, stress relief treatment, if required, is typically performed before removing
the component from the base plate.
4.3 Defects
The common defects associated with SLM components are residual stress, crack
and porosity, among which residual stress can be a major concern for both man-
ufacturing process stability and geometry accuracy (e.g., distortion). Though the
surface roughness of the as-manufactured SLM components is still slightly higher
than that of the conventionally machined surfaces, it is superior to that man-
ufactured via EBM due to smaller laser beam and powder size. Thus, surface
roughness is not discussed in this section.
29
Selective laser melting
4.3.2 Crack
Crack is mostly attributed to the relatively high and localized residual stress, as
mentioned above. By forming and/or expanding the cracks, the residual stresses
is released. On the other hand, Song et al. [115] suggested that the serious
segregation of Nb and Mo at grain boundaries would increase the tendency of
30
Selective laser melting
forming low melting point eutectic phase, and incipient melting might happen
under the complicated thermal condition and form cracks at the grain boundaries.
4.3.3 Porosity
Two types of pores, namely spherical and irregular, are mostly found in as-manufac-
tured SLM components. The spherical pores are attributed to: (a) the inert gas
is involved into the melt pool and (b) the gas trapped inside the powder can not
escape from the melt pool [72, 115]. These spherical pores are less deleterious
to the components’ mechanical properties, while the irregular pores, which can
raise the concentration of stress under service and lead to failure, are the major
concern for controlling the porosities. Thijs et al. [116] suggested that the large
pores with the dimensions of 100∼200 µm result mostly from (a) the accumula-
tions of the powder denudation within the melt pools within a layer, and (b) the
surface roughness across the layers. The balling phenomenon (i.e., the melt pool
is solidified into discontinuous balls due to poor wettability) can also introduce a
large number of irregular pores enclosing non-molten powder and worse surface
roughness [117–119].
• Iron-base alloys: Iron-base alloys are one of the metallic materials widely
applied to SLM at its early phase. The purpose at that early phase was
mainly to understanding the SLM process [120–122], and with the develop-
ment of SLM process the focuses and aims gradually shift to exploring the
possibilities of manufacturing high-value added components. The most com-
monly reported SLM iron-base alloys include 316L stainless steel [123–128].
Other steels, e.g., M2 tool steel [96, 129–131] and 17-4 PH stainless steel
[132–136] have also been reported.
31
Selective laser melting
• Al-Si alloys: Due to their attractive combination of low weight, high heat
conductivity and mechanical properties, Al-Si alloys (AlSi10Mg [151–157]
and Al-12Si [158, 159]) have wide applications in aerospace, automotive in-
dustries as heat exchangers. AlSi10Mg and Al-12Si are hypoeutectic alloys
whose mechanical properties are largely dependant on the morphology of
eutectic silicon. By adding small amount of Mg, Mg2 Si can form and con-
siderably strengthen the matrix without compromising the other mechanical
properties. Manufacturing Al-Si components via SLM is driven by: (a) the
relatively rapid solidification rate associated with SLM process, which can
lead to finer microstructures and more homogeneous distribution of eutectic
silicon to improve the mechanical properties and (b) components’ geometry
design freedom. However, compared to other SLM materials, manufacturing
Al-Si alloys faces different challenges, such as poor flowablitiy of powders,
high reflectivity along with high thermal conductivity and porosities.
32
Selective laser melting
33
Selective laser melting
34
CHAPTER 5
The materials involved in this licentiate research include both EBM IN718 and
SLM IN718. Given the EBM and SLM processes were reviewed in a general sense
in Chapter 3 and 4, a more specific review on the microstructures and mechanical
properties of EBM IN718 and SLM IN718 is provided in this chapter. The idea
here is not to compare one’s superiority to the other, but instead to identify
the missing/controversial part in the published literatures, based on which this
licentiate research is guided to solve these problems.
35
Electron beam melting & selective laser melting IN718
An in situ controlled heat treatment was attempted, by scanning the top surface
of the build after the process was finished, to homogenize and age the microstruc-
ture, but resulted in cracks and poor tensile performance [188]. Efforts have also
been put in identifying process-microstructure relationship, showing that besides
the higher density and better surface finish, the controlled tailoring of grain struc-
tures and crystallographic textures can be achieved by adjusting the scan strategies
[62, 76, 78, 189, 190].
36
CHAPTER 6
Experimental methods
The experimental methods used in the research of this thesis will be present in
this chapter. The EBM IN718 materials were provided by Sandvik Machining So-
lutions AB, Sweden, and the SLM IN718 materials were provided by Siemens AG,
Germany. The post heat treatments, metallographic preparations, microstruc-
ture characterizations, tensile tests and hardness measurements were performed
at Linköping University.
6.1 Materials
6.1.1 EBM IN718
The EBM IN718 was manufactured with an Arcam A2X EBM machine at Sandvik
Machining Solutions AB. The powders used were plasma atomized, with nominal
size ranging from 25 to 106 µm. The chemical composition is given in Table 6.1.
The process parameters were set as suggested by Arcam AB, and the powder bed
temperature (measured from the base plate) was kept at about 1020 ◦ C throughout
the process. The manufacturing batch contained 16 identical blocks. Each block
is dimensioned as in Fig. 6.1a. Note that all these blocks were provided in the
as-manufactured condition, directly removing from the base plate without any
treatment. For more information about this process please refer to appended
paper I.
37
Experimental methods
(a) (b)
Figure 6.1. Schematics of as-manufactured (a) EBM IN718 and (b) SLM IN718 blocks.
Table 6.1. Nominal chemical composition of the Arcam plasma atomized IN718 powder
Element Ni Cr Fe Nb Mo Co Ti Al
wt.% Bal. 19.1 18.5 5.04 2.95 0.07 0.91 0.58
Element Mn Si Cu C P S N O
wt.% 0.05 0.13 0.1 0.035 0.004 0.001 0.0128 0.0133
gas atomized IN718 powder is given in Table 6.2. All the samples were manufac-
tured with an EOS M290 machine equipped with a maximum 400 W Yb-fiber laser.
The process parameters were as recommended by EOS. The components’ longitude
directions are either parallel to or perpendicular to the base plate, designating as
horizontally built and vertically built, respectively. The dimensions are as shown
in Fig. 6.1b. Note that all these blocks were provided in the as-manufactured
condition, directly removing from the base plate without any treatment. For more
information about this process please refer to appended paper III.
Table 6.2. Nominal chemical composition of the gas atomized IN718 powder
Element Ni Cr Fe Nb Mo
wt.% 50∼55 17.0∼21.0 Bal. 4.75∼5.5 2.8∼3.3
Element Co Ti Al Mn Si
wt.% <1.0 0.65∼1.15 0.20∼0.80 <0.35 <0.35
Element Cu C P S B
wt.% <0.3 <0.08 <0.015 <0.0015 <0.006
38
Experimental methods
to 4000 Grit, and polished with diamond suspension from 3 µm to 1/4 µm and
finally with OP-U colloidal silica suspension. Specifically for the SLM IN718, to
reveal the dendritic microstructure, the polished samples were etched for a few
seconds using a 10 ml hydrochloric acid + 1.5 ml 30% hydrogen peroxide etchant.
For transmission electron microscopy characterization, thin foil samples were pre-
pared by mechanically grinding down to 50 µm. To further thin down to electron
transparent, electropolishing was conducted in 10 vol.% perchloric acid + 90 vol.%
Ethanol electrolyte at -20 ◦ C with a Struers TenuPol-5 electrolytic machine, or ion
milling was performed with a Gatan 691 Precision Ion Polishing system.
39
Experimental methods
of tensile test samples please refer to the appended papers. 3∼4 samples were
tested per test condition to obtain acceptable statistics. Tensile tests were con-
ducted under room temperature and open air, using an Instron 5582 universal test
machine with a 100 kN load cell and at a 0.10 %/s strain rate. Since the test sam-
ple was too small to measure strain with extensometer, the strain was measured
using a digital image correlation (DIC) system from Image System AB.
40
CHAPTER 7
Paper I
Microstructure and anisotropic mechanical properties of EBM manu-
factured Inconel 718 and effects of post heat treatments
This paper is partly motivated to investigate the microstructures correspond-
ing to contour and hatching regions and the mechanisms behind the anisotropic
mechanical properties. Tuning the post heat treatment with comparison to the
AMS 5662 specification is also of interested.
The contour microstructure is characterized as heterogeneous grain morpholo-
gies and the overall weak texture, while the hatch region is mostly coarse columnar
41
Summary of included papers
grains elongated along the building direction and has strong ⟨001⟩ building di-
rection texture. The anisotropic tensile properties are observed as higher tensile
strength but lower elongation along the building direction than normal to the
building direction. However, the anisotropy does not seem to result from the
⟨001⟩ building direction texture, but instead is possibly attributed to the align-
ment and distribution of porosities. Since the as-manufactured microstructure has
already be strengthened by the strengthening phases γ ′ /γ ′′ , heat treatments just
slightly increase the strength, and the direct ageing without solution treatment
seems to be the optimum post heat treatment.
Paper II
Height dependent microstructure in Inconel 718 manufactured by Elec-
tron Beam Melting
This paper is a sequel of the first paper, with focus on characterizing the
as-manufactured microstructure gradient along the building direction and ratio-
nalizing the phase evolution during the complex thermal cycles.
Due to the relatively high powder bed temperature and the injection of he-
lium to facilitate cooling after the building process, the as-manufactured IN718
shows a microstructure gradient: from the top surface towards the bottom, the
Laves phase volume fraction increases from about zero, peaks to about 2.3% at 150
µm from the top surface, and decreases gradually to zero again at 1800 µm from
the top surface. The quenched, as-solidified and as-homogenized microstructures
are distinguished within the as-manufactured microstructure. Based on that, the
formation of Laves phase is rationalized with the low cooling rate enabling the
considerable segregation of Nb, which is contradictory to the generally rapid so-
lidification reported in the literatures. 40 minutes of “in-situ” homogenization,
namely soaking in the powder bed before helium is injected, is able to dissolute
completely the Laves phase in as-solidified condition and redistribute homoge-
neously Nb within the matrix. Exceptionally, absence of Laves phase close to the
top surface is attributed to the rapid solidification caused by helium quenching.
Carbide/nitride/carbonitride is less affected by the complex thermal history due to
their highly stability. δ phase is expected to precipitate during the cooling stage,
showing similar evolution as Laves phase. The cooling condition of the cooling
stage also favours the precipitation of γ ′ /γ ′′ throughout the sample, and yields
considerably high strength in the as-manufactured condition.
Paper III
Microstructure and mechanical properties of Inconel 718 produced by
selective laser melting: Sample orientation dependence and effects of
post heat treatments
A aim of this paper is to optimize the post heat treatment for SLM IN718, re-
garding to homogenizing the segregation and correctly precipitating the strength-
ening phases for peak strength. Also this paper is also motivated to uncover the
42
Summary of included papers
43
Summary of included papers
44
CHAPTER 8
Conclusion
The research present in this licentiate thesis focuses on the microstructures and
mechanical properties of IN718 manufactured by EBM and SLM. By addressing
the research questions as mentioned in Chapter Introduction, the following con-
clusions can be made:
• The tensile test shows higher tensile strength but lower elongation along
the building direction than perpendicular to the building direction. The
anisotropy results possibly from the alignment of porosities rather than the
texture.
• Applying heat treatment does not significantly increase the strength since the
strengthening phases γ ′ /γ ′′ have already precipitated in the as-manufactured
condition. Currently, the direct ageing treatment seems to be the optimum
45
Conclusion
for the part free of segregation and Laves phase, while for the whole build
future work is needed to optimize the heat treatment due to the segregation
and Laves phase near the top surface.
For SLM IN718:
• The as-manufactured SLM IN718 has very fine dendritic microstructure and
weak texture, with very fine Laves phase in the interdendrites and without
strengthening phases γ ′ /γ ′′ in the matrix.
• The different accumulations of residual stress are responsible for the “anisotr-
opic”/sample orientation dependent tensile properties, namely the horizon-
tally built samples have higher strength but lower elongation than the ver-
tically build samples.
• Heat treatment is necessary to homogenize the segregation and correctly pre-
cipitate the strengthening phases γ ′ /γ ′′ . With increasing the heat treatment
temperature or holding time the “anisotropy” decreases.
Given this research involves both EBM IN718 and SLM IN718, a comparison
between the microstructures and mechanical properties would be of interest, which
would provide a better overview of both processes. A brief comparison, based on
as-manufactured microstructural and mechanical features, is summarized in the
Table 8.1.
46
Table 8.1. Comparisons of as-manufactured EBM IN718 and SLM IN718 on microstructural and mechanical features
47
Hardness ∼ HV0.3 428 ∼ HV0.3 325
Tensile Aniostropy Yes Yes
Tensile strength BD: 1113 MPa, ⊥ BD: 1002 MPa BD: 989 MPa, ⊥ BD: 1068 MPa
Mechanical property
Elongation BD: 31 %, ⊥ BD: 40 % BD: 35 %, ⊥ BD: 31 %
Tensile properties deviation EBM samples have larger deviation than SLM samples
Strengthening mechanism by γ ′ /γ ′′ by residual strain and dislocations
Surface roughness SLM samples have better surface roughness than EBM samples
• The microstructural and mechanical features of EBM IN718 in this table are specifically from the hatch region.
• Denotation: means parallel to, ⊥ means perpendicular to, BD means building direction.
Conclusion
Conclusion
48
CHAPTER 9
Future work
This licentiate thesis serves as a midterm summary and reflection of the research
progress during the past 2.5 years, as well as a foundation for the next phase of my
Ph.D. journey. Focus will be still on both the EBM IN718 and SLM IN718, but
might shift from the microstructure characterizations and monotonic mechanical
properties to the cyclic mechanical properties, since most of the IN718 applications
involve cyclic loadings.
As indicated in the appended papers, the as-manufactured sample is not at the
peak aged condition, which needs heat treatment improve the strength, for both
EBM and SLM IN718. Heat treatment can significantly affect the precipitation
or dissolution of certain precipitates. The effects of precipitates on fatigue crack
propagation behaviours are of interest, but so far have been rarely reported. On
the other hand, specifically for EBM IN718, the columnar grain boundaries are
mostly parallel to the building direction, and the grain boundaries’ role on crack
propagation would be studied under loading that is either parallel or perpendicular
to building direction.
4-point bending fatigue test is also planned to investigate the crack initiation
behaviours on machined samples at HIPed and un-HIPed, heat treated and un-heat
treated conditions for both EBM and SLM IN718.
49
Future work
50
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Part Part II:
Included papers
知不知上,不知知病。
夫唯病病,是以不病。
聖人不病,以其病病,是以不病。
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69
Papers
The papers associated with this thesis have been removed for
copyright reasons. For more details about these see:
http://urn.kb.se/resolve?urn=urn:nbn:se:liu:diva-144491
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